CN108048789B - Double-phase stainless steel plasma anode nitriding surface strengthening process - Google Patents
Double-phase stainless steel plasma anode nitriding surface strengthening process Download PDFInfo
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- CN108048789B CN108048789B CN201711069019.1A CN201711069019A CN108048789B CN 108048789 B CN108048789 B CN 108048789B CN 201711069019 A CN201711069019 A CN 201711069019A CN 108048789 B CN108048789 B CN 108048789B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
- C23C8/38—Treatment of ferrous surfaces
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
- C23C8/26—Nitriding of ferrous surfaces
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
Abstract
The invention discloses a double-phase stainless steel plasma anode nitriding surface strengthening technology, which comprises the following steps: (1) pretreating the surface of the duplex stainless steel; (2) plasma-assisted anode nitridation: performing surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, and putting the duplex stainless steel subjected to surface pretreatment into an anode nitriding device for nitriding treatment; (3) and (6) annealing. The invention can effectively inhibit the formation of brittle phases, enables the surface layer to the core of the disc to have excellent toughness matching, reduces the secondary deformation of a workpiece caused by temperature gradient on the basis of ensuring uniform structure and excellent mechanical property as much as possible, simultaneously can avoid coarsening damage to the treated surface caused by ' arcing ' and ' edge effect ' and the like, is beneficial to the formation of a white and bright metastable compound S phase, inhibits the precipitation of brittle phases such as epsilon-Fe 2-3N and gamma ' -Fe4N and enables the disc to have higher hardness, wear resistance and corrosion resistance.
Description
Technical Field
The invention relates to a metal surface strengthening technology, in particular to a plasma anode nitriding surface strengthening process technology of duplex stainless steel, which adopts a plasma-assisted anode nitriding technology to carry out surface modification and strengthening treatment on an ultra-low carbon duplex stainless steel disc.
Background
At present, a domestic starch separator is a nozzle continuous discharge type disc separator, is mainly used for starch refining, pre-concentration, protein separation, starch recovery and the like in the starch industry, and can also be used for the technical processes of liquid-solid two-phase separation, concentration recovery, clarification and the like in the departments of food, medicine, dyeing, environmental protection and the like, such as the recovery of kaolin, paper pulp, wastewater treatment and the like. The time for manufacturing the disc-type starch separator is short in China, and the main technology is obtained by digesting and absorbing similar products abroad. The rotary drum component of the disc type starch separator manufactured in China at present is composed of a plurality of parts, the internal structure is complex, the assembly is complex, the feeding system is easy to block, the equipment needs to be stopped for cleaning the rotary drum after running for ten days, the three-phase separation cannot be realized, and the working efficiency of the equipment is greatly reduced. The advanced western countries have earlier research in the field of solid-liquid separation, the current technology is comprehensive and complete, and a large number of examples of commercial application exist, but the products of the companies are extremely expensive, the equipment maintenance is troublesome, and the cost is relatively high.
The large-scale, intelligent, multifunctional, high-speed, high-precision and material application of the disc type starch separator is a future development trend, and the latest development direction of the domestic starch separator is inevitably the update of the disc type starch separator product. The material is an important aspect for researching new products of the disc type starch separator, and is concerned by many researchers, wherein the research on the surface modification and strengthening process of the duplex stainless steel improves the application capability of the duplex stainless steel in the large disc type separator, is one of the foundation for the future generation of the products of the disc type starch separator, and is one of the development directions of the duplex stainless steel for the parts of the disc type separator.
Disclosure of Invention
The invention aims to provide a plasma anode nitriding surface strengthening process for duplex stainless steel, which adopts a plasma-assisted anode nitriding technology to carry out surface modification and strengthening treatment on an ultra-low carbon duplex stainless steel disc.
The invention relates to a double-phase stainless steel plasma anode nitriding surface strengthening process, which adopts the technical scheme that the process comprises the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: degreasing, cleaning with an industrial cleaning agent, washing with water and drying;
(2) plasma-assisted anode nitridation: performing surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the argon partial pressure is 0.05-0.75Pa, the nitrogen partial pressure is 0.5-750Pa, the bias voltage is 35-2000V, the nitriding temperature is 200-350 ℃, and the nitriding time is 1-3.5 hours;
(3) annealing: annealing the plasma-assisted anode nitrided surface strengthened duplex stainless steel in the gas atmosphere or vacuum environment, wherein the annealing temperature is controlled within the range of 500-1100 ℃, and the annealing rate is controlled within the range of 5-100 ℃/s.
Preferably, the plasma-assisted technique described in step (2) is based on argon gas generation in a low-pressure apparatus, wherein the ionization voltage is controlled between 20-40V and the ionization current is controlled between 10-180A.
Preferably, the nitrogen source in the anode nitriding apparatus in step (2) may be nitrogen gas, ammonia gas, or a mixed gas of the two.
Preferably, the gas atmosphere in step (3) may be one or more of nitrogen and argon, or may be a mixed gas atmosphere of the gas atmosphere and one or more of hydrogen and ammonia.
Preferably, the nitriding temperature and the temperature gradient of the nitriding treatment method are low, the additional deformation of the disc and the rotary drum caused by nitriding treatment can be effectively reduced, and the surface-strengthened duplex stainless steel is particularly suitable for a duplex stainless steel large separator disc with corn oil, water, sediment and other media.
Compared with the traditional nitriding technology, the invention has the advantages that:
(1) the nitriding process parameters are matched, so that the formation of brittle phases can be effectively inhibited, and the surface layer of the disk has excellent toughness matching with the core part. Meanwhile, on the basis of ensuring uniform structure and excellent mechanical property, the secondary deformation of the workpiece caused by temperature gradient is reduced as much as possible.
(2) The nitriding treatment method disclosed by the invention is low in temperature, short in period and thick and uniform in a nitriding layer, can avoid coarsening damage to the treated surface caused by arc striking, edge effect and the like, and aggravate frictional wear, and can be beneficial to formation of a white and bright metastable compound S phase and inhibition of precipitation of brittle phases such as epsilon-Fe 2-3N and gamma' -Fe4N, so that the disc has high hardness, wear resistance and corrosion resistance;
(3) the nitriding temperature and the temperature gradient of the nitriding treatment method are low, the additional deformation of the disc and the rotary drum caused by nitriding treatment can be effectively reduced, and the surface-strengthened duplex stainless steel is particularly suitable for a duplex stainless steel large separator disc of corn oil, water, sediment and other media.
Detailed Description
In order to better illustrate the invention, the following examples are given. It should be emphasized that the examples are not meant to limit the scope of the invention to the conditions described in the examples, which are intended to further illustrate the content of the invention and its feasibility.
Example 1:
a duplex stainless steel plasma anode nitriding surface strengthening process adopts the technical scheme that the process comprises the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: firstly, carrying out degreasing treatment on the duplex stainless steel by using a trichloroethylene solvent, then soaking and cleaning the duplex stainless steel for 10 minutes at 90 ℃ by using an industrial cleaning agent, then washing the duplex stainless steel by using water, and drying the duplex stainless steel at 93 ℃ to obtain the duplex stainless steel with the surface being pretreated;
(2) plasma-assisted anode nitridation: performing surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the argon partial pressure is 0.5Pa, the nitrogen partial pressure is 500Pa, the bias voltage is 800V, the nitriding temperature is 250 ℃, and the nitriding time is 1.5 hours;
(3) annealing: and (3) annealing the plasma-assisted anode nitrided surface strengthened duplex stainless steel in the step (2) in a nitrogen atmosphere, wherein the annealing temperature is controlled at 800 ℃, and the annealing rate is controlled at 45 ℃/s.
Example 2:
a duplex stainless steel plasma anode nitriding surface strengthening process adopts the technical scheme that the process comprises the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: degreasing duplex stainless steel by using an ethyl caproate solvent, soaking and cleaning for 15 minutes at 83 ℃ by using an industrial cleaning agent, washing with water, and drying at 70 ℃ to obtain the duplex stainless steel with the surface pretreated;
(2) plasma-assisted anode nitridation: carrying out surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the argon partial pressure is 0.05Pa, the ammonia partial pressure is 150Pa, the bias voltage is 200V, the nitriding temperature is 200 ℃, and the nitriding time is 1 hour;
(3) annealing: and (3) annealing the plasma-assisted anode nitrided surface reinforced duplex stainless steel in the atmosphere of nitrogen and argon (volume ratio of 1: 1) in the step (2), wherein the annealing temperature is controlled at 1100 ℃, and the annealing rate is controlled at 80 ℃/s.
Example 3:
a duplex stainless steel plasma anode nitriding surface strengthening process adopts the technical scheme that the process comprises the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: firstly, degreasing duplex stainless steel by using an acetone solvent, then soaking and cleaning the duplex stainless steel for 15 minutes at 70 ℃ by using an industrial cleaning agent, washing the duplex stainless steel by using water, and drying the duplex stainless steel at 93 ℃ to obtain the duplex stainless steel with the surface pretreated;
(2) plasma-assisted anode nitridation: performing surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the partial pressure of argon is 0.3Pa, the partial pressure of nitrogen and ammonia (the volume ratio is 2: 1) is 0.5Pa, the voltage is biased to 35V, the nitriding temperature is 300 ℃, and the nitriding time is 1.5 hours;
(3) annealing: and (3) annealing the plasma-assisted anode nitrided surface strengthened duplex stainless steel in the argon atmosphere, wherein the annealing temperature is controlled to be 780 ℃, and the annealing rate is controlled to be 40 ℃/s.
Example 4:
a duplex stainless steel plasma anode nitriding surface strengthening process adopts the technical scheme that the process comprises the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: degreasing duplex stainless steel by using an ethyl acetate solvent, then soaking and cleaning for 12 minutes at 85 ℃ by using an industrial cleaning agent, washing with water, and drying at 85 ℃ to obtain the duplex stainless steel with the surface pretreated;
(2) plasma-assisted anode nitridation: carrying out surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the argon partial pressure is 0.4Pa, the nitrogen and ammonia (volume ratio is 1: 1) partial pressure is 750Pa, the bias voltage is 1900V, the nitriding temperature is 280 ℃, and the nitriding time is 2 hours;
(3) annealing: and (3) annealing the plasma-assisted anode nitrided surface reinforced duplex stainless steel in the step (2) in the atmosphere of nitrogen, argon and hydrogen (the volume ratio is 2: 1), wherein the annealing temperature is controlled at 500 ℃, and the annealing rate is controlled at 10 ℃/s.
Example 5:
a duplex stainless steel plasma anode nitriding surface strengthening process adopts the technical scheme that the process comprises the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: degreasing duplex stainless steel by using an acetone solvent, soaking and cleaning the duplex stainless steel for 5 minutes at 90 ℃ by using an industrial cleaning agent, washing the duplex stainless steel by using water, and drying the washed duplex stainless steel at 70 ℃ to obtain the duplex stainless steel with the surface pretreated;
(2) plasma-assisted anode nitridation: performing surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the argon partial pressure is 0.75Pa, the nitrogen partial pressure is 300Pa, the bias voltage is 650V, the nitriding temperature is 350 ℃, and the nitriding time is 1.2 hours;
(3) annealing: and (3) annealing the plasma-assisted anode nitrided surface strengthened duplex stainless steel in the atmosphere of nitrogen and argon (volume ratio is 3: 1), wherein the annealing temperature is controlled at 1000 ℃, and the annealing rate is controlled at 100 ℃/s.
Example 6:
a duplex stainless steel plasma anode nitriding surface strengthening process adopts the technical scheme that the process comprises the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: firstly, degreasing duplex stainless steel by using a trichloroethylene solvent, then soaking and cleaning for 10 minutes at 80 ℃ by using an industrial cleaning agent, then washing with water, and drying for 30 minutes at 40 ℃ in warm air to obtain the duplex stainless steel with the surface pretreated;
(2) plasma-assisted anode nitridation: carrying out surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the argon partial pressure is 0.2Pa, the ammonia partial pressure is 100Pa, the bias voltage is 300V, the nitriding temperature is 300 ℃, and the nitriding time is 3 hours;
(3) annealing: and (3) annealing the plasma-assisted anode nitrided surface reinforced duplex stainless steel in the step (2) in the atmosphere of nitrogen, argon and ammonia (the volume ratio is 1: 2), wherein the annealing temperature is controlled at 650 ℃, and the annealing rate is controlled at 5 ℃/s.
Claims (5)
1. A plasma anode nitriding surface strengthening process for duplex stainless steel is characterized by comprising the following steps:
(1) surface pretreatment of duplex stainless steel: the main process comprises the following steps: degreasing, cleaning with an industrial cleaning agent, washing with water and drying;
(2) plasma-assisted anode nitridation: performing surface modification and strengthening treatment on the ultra-low carbon duplex stainless steel disc by adopting a plasma-assisted anode nitriding technology, putting the duplex stainless steel subjected to surface pretreatment in the step (1) into an anode nitriding device, and controlling nitriding process parameters, wherein the argon partial pressure is 0.05-0.75Pa, the nitrogen partial pressure is 0.5-750Pa, the bias voltage is 35-2000V, the nitriding temperature is 200-350 ℃, and the nitriding time is 1-3.5 hours;
(3) annealing: annealing the plasma-assisted anode nitrided surface strengthened duplex stainless steel in the gas atmosphere or vacuum environment, wherein the annealing temperature is controlled within the range of 500-1100 ℃, and the annealing rate is controlled within the range of 5-100 ℃/s.
2. A duplex stainless steel plasma anode nitriding surface strengthening process according to claim 1, wherein the plasma assisted technique of step (2) is based on argon gas generation in a low pressure device, wherein the ionization voltage is controlled between 20-40V and the ionization current is controlled between 10-180A.
3. The plasma anodic nitridation surface enhancement process of claim 1, wherein the nitrogen source in the anodic nitridation device of step (2) is nitrogen, ammonia, or a mixture thereof.
4. A duplex stainless steel plasma anode nitriding surface strengthening process according to claim 1, wherein the gas atmosphere in step (3) can be one or more of nitrogen and argon.
5. The plasma anodic nitridation surface strengthening process for duplex stainless steel according to claim 1, wherein said nitridation treatment method reduces additional deformation of disks and drums caused by nitridation treatment, and the surface-strengthened duplex stainless steel is suitable for a large separator disk of duplex stainless steel containing corn oil, water and sediment media.
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